CN113337014A - Preparation of PVA/cassava starch/LAE/anthocyanin intelligent chromogenic active composite membrane and application of PVA/cassava starch/LAE/anthocyanin intelligent chromogenic active composite membrane in packaging bacteriostasis - Google Patents
Preparation of PVA/cassava starch/LAE/anthocyanin intelligent chromogenic active composite membrane and application of PVA/cassava starch/LAE/anthocyanin intelligent chromogenic active composite membrane in packaging bacteriostasis Download PDFInfo
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- CN113337014A CN113337014A CN202110448563.7A CN202110448563A CN113337014A CN 113337014 A CN113337014 A CN 113337014A CN 202110448563 A CN202110448563 A CN 202110448563A CN 113337014 A CN113337014 A CN 113337014A
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- anthocyanin
- pva
- lae
- starch
- composite membrane
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Links
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Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B65—CONVEYING; PACKING; STORING; HANDLING THIN OR FILAMENTARY MATERIAL
- B65D—CONTAINERS FOR STORAGE OR TRANSPORT OF ARTICLES OR MATERIALS, e.g. BAGS, BARRELS, BOTTLES, BOXES, CANS, CARTONS, CRATES, DRUMS, JARS, TANKS, HOPPERS, FORWARDING CONTAINERS; ACCESSORIES, CLOSURES, OR FITTINGS THEREFOR; PACKAGING ELEMENTS; PACKAGES
- B65D65/00—Wrappers or flexible covers; Packaging materials of special type or form
- B65D65/38—Packaging materials of special type or form
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2303/00—Characterised by the use of starch, amylose or amylopectin or of their derivatives or degradation products
- C08J2303/02—Starch; Degradation products thereof, e.g. dextrin
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/05—Alcohols; Metal alcoholates
- C08K5/053—Polyhydroxylic alcohols
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/04—Oxygen-containing compounds
- C08K5/15—Heterocyclic compounds having oxygen in the ring
- C08K5/151—Heterocyclic compounds having oxygen in the ring having one oxygen atom in the ring
- C08K5/1545—Six-membered rings
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Mechanical Engineering (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention provides a preparation method of a PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite film and application of the PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite film in packaging and bacteriostasis, and belongs to the technical field of food packaging materials. The composite film can better prevent ultraviolet rays and visible light from transmitting and is beneficial to preventing degradation and oxidation of food; the obtained composite film has high water absorption rate and water vapor transmission rate and good fresh-keeping effect; the food packaging material can present different colors under different pH values, has safe components and no toxic or side effect, and can ensure that the freshness of the packaged food has visual phenomenon.
Description
Technical Field
The invention belongs to the technical field of food packaging materials, and particularly relates to a preparation method of a PVA/cassava starch/LA/anthocyanin intelligent chromogenic active composite membrane and application thereof in packaging bacteriostasis.
Background
The smart package is a new type of food package, and consumers can evaluate the quality and freshness of food by its color change, which is defined by european law as a material and article for detecting the condition of packaged food or the surrounding environment of food. When the food is deteriorated, the pH value changes, and the quality and freshness of the food in the package can be monitored in real time by adding the pH indicator into the packaging material. pH indicators include chlorophenol red, bromophenol blue, bromocresol green, and the like, but these synthetic chemical agents have potential effects on human health, and therefore should be avoided in smart package development and production. The anthocyanin belongs to flavonoid substances (phenolic phytochemicals), is a plant secondary metabolite, widely exists in colored plant flowers, stems, leaves and fruits, is a renewable, safe and nontoxic natural pigment, can be dissolved in water, methanol and ethanol, can change color within a wide pH value range, and is widely applied to intelligent packaging research and development.
Many researchers have studied the effect of different anthocyanins on film performance. Qin et al prepared PVA/starch films containing anthocyanins and betacyanins, found that both anthocyanins can improve the performance of the films on ultraviolet and visible light blocking, water resistance, oxidation resistance and the like, and that betacyanins can improve the compactness of the films compared with anthocyanins. Chen et al prepared curcumin and purple sweet potato anthocyanin film, test results show that the two additives have no obvious influence on the water solubility, water vapor transmission rate and other properties of the film, and the film can change color obviously along with fish deterioration in fish freshness detection experiments. Jiang Guang Yanang et al prepared composite films with different base materials containing purple sweet potato anthocyanin found through comparison that the highest tensile strength of the potato starch/sodium carboxymethyl cellulose film containing anthocyanin was about 15.39MPa, and the highest elongation at break of the potato starch/konjac glucomannan film was about 44.79 MPa. The PVA/purple sweet potato starch composite film containing purple sweet potato anthocyanin is prepared by Zhongxiao et al, and researches show that the mechanical property of the film is improved by adding the purple sweet potato anthocyanin, the freshness of milk can be detected, and the color of the film is gradually changed from light purple to light red along with the gradual deterioration of the milk.
Various anthocyanins have been used in the preparation of active packaging, such as roselle anthocyanins, blueberry anthocyanins, lycium ruthenicum anthocyanins, myricetin, black carrot anthocyanins, purple potato anthocyanins, etc., and studies have indicated that the anthocyanins types have different effects on film performance.
At present, researches on mulberry anthocyanin/PVA/cassava starch intelligent films are few, and the performance influence of the anthocyanin/LAE-containing PVA/cassava starch intelligent active films (LAC films) is not completely clear, so in order to research an intelligent color-developing composite film with better antibacterial performance and higher safety, the influence of anthocyanin content on the preparation and performance of the LAC composite film, and the in-vitro antibacterial performance and mechanism of the LAC composite film need to be researched.
Disclosure of Invention
In order to solve the technical problems, the invention provides a preparation method of a PVA/cassava starch/LAE/anthocyanin intelligent chromogenic active composite membrane and an application thereof in packaging bacteriostasis, wherein the composite membrane can present different colors under different pH values, so that the freshness of packaged food can be visualized; the food preservative has the advantages of favorable food degradation and oxidation prevention, good preservation effect, favorable antibacterial activity and high safety.
In order to achieve the purpose, the invention provides the following technical scheme:
a preparation method of a PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite membrane comprises the steps of gelatinizing cassava starch, mixing with a PVA solution and glycerol, adding LAE with the total mass being 1-5% by weight and anthocyanin with the total mass being 5-50% by weight, stirring and mixing uniformly under the heating condition of a constant-temperature water bath to obtain a membrane casting solution, and finally carrying out a tape casting method on the membrane casting solution to obtain a finished product composite membrane.
Further, the preparation method of the PVA/cassava starch/LAE/anthocyanin intelligent color development active composite membrane specifically comprises the following steps:
(1) gelatinized tapioca starch
Adding cassava starch into deionized water to prepare a starch suspension with the mass concentration of 10-11%; putting the starch suspension into a constant-temperature water bath environment, heating to 81-84 ℃, and stirring for 30-35 min until the starch suspension is completely gelatinized to obtain gelatinized starch for later use;
(2) preparation of PVA solution
Putting PVA into deionized water according to a certain solid-liquid ratio, placing the PVA into a constant-temperature water bath environment, heating to 98-100 ℃, and stirring for 54-58 min until the PVA is completely dissolved to obtain a PVA solution with the concentration of 10-11%;
(3) preparing casting solution
Mixing gelatinized starch and a PVA solution according to a volume ratio of 70: 30-32 to obtain a mixture 1, adding glycerol into the mixture 1 to obtain a mixture 2, placing the mixture 2 in a constant-temperature water bath environment, heating to 81-84 ℃, and stirring for 30-35 min to uniformly mix the solutions to obtain a mixed solution for later use;
adding LAE accounting for 1-5 wt% of the total mass of the mixed solution and anthocyanin accounting for 5-50 wt% of the total mass of the mixed solution, continuing stirring in a constant-temperature water bath environment at 23-25 ℃ for 30-33 min until all components are uniformly mixed, taking out, and placing in an ultrasonic environment to vibrate at normal temperature for 4-5 min to obtain the membrane casting solution;
(4) casting film by tape casting method
Pouring the casting solution into a mould by adopting a tape casting method for casting, then placing the mould in a constant temperature environment for drying and demoulding to obtain a composite membrane, and sealing and storing the composite membrane.
Further, the composite film has a thickness of 0.11-0.18 mm, a tensile strength of 11.25-24.43 MPa, an elongation at break of 103-439%, a light transmittance at 200nm of 0, an opacity of 4.11-11.01, a water absorption of 15.79-17.65%, and a water vapor transmission rate of 1.00 x 10-11～1.62×10-11g·m-1·s-1·Pa-1。
Further, the stirring is carried out at a speed of 425 to 430 r/min.
Further, the addition amount of the glycerol is 18-20% of the total dry weight of the mixture 1.
Further, the anthocyanin is mulberry anthocyanin; and (3) adding anthocyanin in an amount which is 5 percent of the total mass of the mixed solution.
Further, in the step (4), the drying temperature is 25-28 ℃, and the drying time is 24 hours.
The invention provides a PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite membrane prepared by any one of the preparation methods.
The invention provides an application of the PVA/cassava starch/LAE/anthocyanin intelligent chromogenic active composite membrane in packaging bacteriostasis, wherein the composite membrane has bacteriostasis to escherichia coli and staphylococcus aureus, and can be applied to packaging materials in food and medicine products.
The invention has the following beneficial effects:
1. PVA used in the composite film has better compatibility with cassava starch, LAE is added to change the microscopic morphology of the composite film, and the thickness of the LAE film is not obviously influenced; according to the invention, the synergistic plasticization effect of LAE aggregation and glycerol is utilized, so that the tensile strength of the obtained composite film is slightly reduced, but the elongation at break is remarkably increased, the tensile strength is 11.25-24.43 MPa, and the elongation at break is 103-439%; the anthocyanin is added, so that the food can be in different colors under different pH values, is safe in components and free of toxic and side effects, and the freshness of the packaged food can be visualized.
2. The composite film has lower ultraviolet transmittance and higher transparency, not only can protect the quality and flavor of food, but also is beneficial to better displaying the food to consumers; the composite film can better prevent ultraviolet rays and visible light from transmitting and is beneficial to preventing degradation and oxidation of food; the added anthocyanin is agglomerated, the structural integrity of the film is damaged, the transmission of water molecules is promoted, the water vapor transmission rate is slightly increased, and the fresh-keeping effect is better.
3. The composite membrane has antibacterial activity on escherichia coli and staphylococcus aureus, and the added LAE changes the membrane potential and permeability of cells to increase the permeability of bacterial cell membranes and further cause the leakage of the contents of the bacterial cell membranes, so that the sterilization effect is realized;
4. the intelligent color developing film disclosed by the invention has an antibacterial effect and a good color developing effect, the problem of conflict between the antibacterial effect and the good color developing effect is solved by reasonably controlling the consumption of the raw materials, the anthocyanin can be used for displaying different colors under different pH values, the freshness of food packaged in the composite film can be visualized, and when milk is packaged, the purple gray color can be changed into purple red color in the spoiled milk, so that the good color developing effect is achieved.
5. The tapioca starch used as the raw material has more amylopectin content, is easy to form a film in the manufacturing process, reduces the operation difficulty, and can play a role in plasticizing by adding glycerol and improve the plasticity of a packaging film; meanwhile, the two groups of components are safe, are suitable for the field of food processing, are favorable for reducing the production cost and are suitable for popularization and use.
Drawings
FIG. 1 is an SEM photograph of each composite membrane (in the drawing, a-j are a control group, examples 1-4 groups, a blank group, and comparative examples 1-4 groups in this order).
FIG. 2 is an infrared spectrum of each composite film (in the figure, a-j are a control group, examples 1-4 groups, a blank group and comparative examples 1-4 groups in sequence).
FIG. 3 shows the X-ray diffraction patterns of the composite films (in the figure, a-j are a control group, examples 1-4 groups, a blank group and comparative examples 1-4 groups in sequence).
FIG. 4 shows the shielding of the color disk by each set of composite films. (in the figure, a and g are the case without a shielding material; b-f are a blank group and comparative examples 1-4 in sequence; and h-l are a control group and examples 1-4 in sequence).
FIG. 5 shows the inhibition zones of the composite membranes of each group against Escherichia coli (in the figure, a-j are a control group, examples 1-4 groups, a blank group and comparative examples 1-4 groups in sequence).
FIG. 6 shows the inhibition zones of the composite membranes of each group against Staphylococcus aureus (in the figure, a-j are a control group, examples 1-4 groups, a blank group, and comparative examples 1-4 groups in sequence).
FIG. 7 shows the color change of the anthocyanin solution at different pH values (from left to right, in order, pH 2-11).
FIG. 8 anthocyanin/LAE solutions changed color at different pH values (pH 2-11 from left to right).
FIG. 9 is a graph of the color change of the composite membrane of comparative example 1 at different pH values.
FIG. 10 the color of the composite membrane of example 1 of the present invention changed at different pH values.
FIG. 11 initial color of milk before soaking experiment (in the figure, a-j are blank group, comparative example 1-4 group, control group, example 1-4 group in sequence).
FIG. 12 color profiles of the membranes from each group were taken out after the soaking test (in the figure, a-j are blank group, comparative examples 1-4 group, control group, and examples 1-4 group in order).
FIG. 13 shows the color change of milk after soaking test (in the figure, a-j are blank group, comparative example 1-4 group, control group, and example 1-4 group in sequence).
Detailed Description
The following examples may assist those skilled in the art in a more complete understanding of the present invention, but are not intended to limit the invention in any way. The raw materials used in the invention are as follows: polyvinyl alcohol (PVA) is 1750 +/-50, the purity of lauroyl arginine ethyl ester hydrochloride (LAE) is 98%, tapioca starch is food grade, mulberry anthocyanin food grade (content is 25%), and glycerol (glycerin) are all purchased from chemical raw materials and medicinal raw material companies. Escherichia coli and Staphylococcus aureus were purchased from Shanghai Lu Microscience and technology Co. Trypticase Soytone agar Medium (TSA), trypticase Soytone liquid Medium (TSB) were purchased from Kyoto Kyowa Microbiol technology, Inc.
Example 1
The preparation method of the PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite membrane specifically comprises the following steps:
(1) gelatinized tapioca starch
Adding cassava starch into deionized water to prepare a starch suspension with the mass concentration of 10%; putting the starch suspension into a constant-temperature water bath environment, heating to 81 ℃, and stirring for 30min until the starch suspension is completely gelatinized to obtain gelatinized starch for later use; the stirring is carried out at a speed of 425 r/min;
(2) preparation of PVA solution
Putting PVA into deionized water according to a certain solid-liquid ratio, placing the PVA into a constant-temperature water bath environment, heating to the temperature of 98 ℃, and stirring for 54min until the PVA is completely dissolved to obtain a 10% PVA solution; the stirring is carried out at a speed of 425 r/min;
(3) preparing casting solution
Mixing gelatinized starch and PVA solution according to a volume ratio of 70:30 to obtain a mixture 1, adding glycerol into the mixture 1 to obtain a mixture 2, placing the mixture 2 in a constant-temperature water bath environment, heating to 81 ℃, and stirring for 30min to uniformly mix the solution to obtain a mixed solution for later use; the glycerol was added in an amount of 18% of the total dry weight of mixture 1;
adding LAE accounting for 5% of the total mass of the mixed solution and anthocyanin accounting for 5% of the total mass of the mixed solution, continuing stirring in a constant-temperature water bath environment at 23 ℃ for 30min until all components are uniformly mixed, taking out the mixed solution, and placing the mixed solution in an ultrasonic environment with the frequency of 28KHz to vibrate at normal temperature for 4min to obtain the membrane casting solution; the stirring is carried out at a speed of 425 r/min;
(4) casting film by tape casting method
Pouring the casting solution into a mold by adopting a tape casting method for casting, then placing the mold in a constant temperature environment for drying and demolding to obtain a composite film, and sealing and storing the composite film; the drying temperature is 25 ℃, and the drying time is 24 h.
Example 2
The preparation method of the PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite membrane specifically comprises the following steps:
(1) gelatinized tapioca starch
Adding cassava starch into deionized water to prepare a starch suspension with the mass concentration of 11%; putting the starch suspension into a constant-temperature water bath environment, heating to 84 ℃, and stirring for 35min until the starch suspension is completely gelatinized to obtain gelatinized starch for later use; the stirring is carried out at the speed of 430 r/min;
(2) preparation of PVA solution
Putting PVA into deionized water according to a certain solid-liquid ratio, placing the PVA in a constant-temperature water bath environment, heating to 100 ℃, and stirring for 58min until the PVA is completely dissolved to obtain a PVA solution with the concentration of 11%; the stirring is carried out at the speed of 430 r/min;
(3) preparing casting solution
Mixing gelatinized starch and PVA solution according to a volume ratio of 70:32 to obtain a mixture 1, adding glycerol into the mixture 1 to obtain a mixture 2, placing the mixture 2 in a constant-temperature water bath environment, heating to 84 ℃, and stirring for 35min to uniformly mix the solution to obtain a mixed solution for later use; the glycerol was added in an amount of 20% of the total dry weight of mixture 1;
adding LAE accounting for 1 weight percent of the total mass of the mixed solution and anthocyanin accounting for 20 weight percent of the total mass of the mixed solution, continuously stirring for 33min in a constant-temperature water bath environment at 25 ℃ until all components are uniformly mixed, taking out the mixed solution, and placing the mixed solution in an ultrasonic environment with the frequency of 30KHz to vibrate at normal temperature for 5min to obtain the membrane casting solution; the stirring is carried out at the speed of 430 r/min;
(4) casting film by tape casting method
Pouring the casting solution into a mold by adopting a tape casting method for casting, then placing the mold in a constant temperature environment for drying and demolding to obtain a composite film, and sealing and storing the composite film; the drying temperature is 28 ℃, and the drying time is 24 h.
Example 3
The preparation method of the PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite membrane specifically comprises the following steps:
(1) gelatinized tapioca starch
Adding cassava starch into deionized water to prepare a starch suspension with the mass concentration of 10.5%; putting the starch suspension into a constant-temperature water bath environment, heating to 82 ℃, and stirring for 31min until the starch suspension is completely gelatinized to obtain gelatinized starch for later use; the stirring is carried out at a speed of 428 r/min;
(2) preparation of PVA solution
Putting PVA into deionized water according to a certain solid-liquid ratio, placing the PVA in a constant-temperature water bath environment, heating to 99 ℃, and stirring for 55min until the PVA is completely dissolved to obtain a PVA solution with the concentration of 10.5%; the stirring is carried out at a speed of 428 r/min;
(3) preparing casting solution
Mixing gelatinized starch and PVA solution according to a volume ratio of 70:31 to obtain a mixture 1, adding glycerol into the mixture 1 to obtain a mixture 2, placing the mixture 2 in a constant-temperature water bath environment, heating to 82 ℃, and stirring for 31min to uniformly mix the solution to obtain a mixed solution for later use; the glycerol was added in an amount of 19% of the total dry weight of mixture 1;
adding LAE accounting for 4% of the total mass of the mixed solution and anthocyanin accounting for 35% of the total mass of the mixed solution, continuing stirring in a constant-temperature water bath environment at 24 ℃ for 31min until all components are uniformly mixed, taking out the mixed solution, and placing the mixed solution in an ultrasonic environment with the frequency of 29KHz to vibrate at normal temperature for 4.5min to obtain the membrane casting solution; the stirring is carried out at a speed of 428 r/min;
(4) casting film by tape casting method
Pouring the casting solution into a mold by adopting a tape casting method for casting, then placing the mold in a constant temperature environment for drying and demolding to obtain a composite film, and sealing and storing the composite film; the drying temperature is 26 ℃, and the drying time is 24 h.
Example 4
The preparation method of the PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite membrane specifically comprises the following steps:
(1) gelatinized tapioca starch
Adding cassava starch into deionized water to prepare a starch suspension with the mass concentration of 10%; putting the starch suspension into a constant-temperature water bath environment, heating to 81 ℃, and stirring for 30min until the starch suspension is completely gelatinized to obtain gelatinized starch for later use; the stirring is carried out at the speed of 430 r/min;
(2) preparation of PVA solution
Putting PVA into deionized water according to a certain solid-liquid ratio, placing the PVA in a constant-temperature water bath environment, heating to 100 ℃, and stirring for 58min until the PVA is completely dissolved to obtain a 10% PVA solution; the stirring is carried out at the speed of 430 r/min;
(3) preparing casting solution
Mixing gelatinized starch and PVA solution according to a volume ratio of 70:30 to obtain a mixture 1, adding glycerol into the mixture 1 to obtain a mixture 2, placing the mixture 2 in a constant-temperature water bath environment, heating to 81 ℃, and stirring for 30min to uniformly mix the solution to obtain a mixed solution for later use; the glycerol was added in an amount of 20% of the total dry weight of mixture 1;
adding LAE accounting for 5% of the total mass of the mixed solution and anthocyanin accounting for 50% of the total mass of the mixed solution, continuing stirring in a constant-temperature water bath environment at 25 ℃ for 30min until all components are uniformly mixed, taking out the mixed solution, and placing the mixed solution in an ultrasonic environment with the frequency of 28KHz to vibrate at normal temperature for 5min to obtain the membrane casting solution; the stirring is carried out at the speed of 430 r/min;
(4) casting film by tape casting method
Pouring the casting solution into a mold by adopting a tape casting method for casting, then placing the mold in a constant temperature environment for drying and demolding to obtain a composite film, and sealing and storing the composite film; the drying temperature is 25 ℃, and the drying time is 24 h.
Control group: no anthocyanins were added, the rest being identical to example 1.
Blank group: the procedure of example 1 was repeated except that no anthocyanins or LAE was added.
Comparative example 1: no LAE was added and the rest was identical to example 1.
Comparative example 2: no LAE was added and the rest was identical to example 2.
Comparative example 3: no LAE was added and the rest was identical to example 3.
Comparative example 4: no LAE was added and the rest was identical to example 4.
The following tests were performed for examples 1-4 and the blank set:
1. observation by scanning electron microscope
The cross section of the sample which is broken in the mechanical property test is used as a sample for observation, and the sample is stuck on a sample table by a conductive adhesive tape. Spraying gold powder in a vacuum sampling machine, taking out, and observing under 2kV voltage and 2000 times magnification. The results are shown in FIG. 1.
Fig. 1 is an SEM photograph of each set of composite films. As can be seen in FIG. 1, the blank group has a smooth and uniform cross section, which indicates that PVA and tapioca starch have good compatibility and form a hydrogen bond; the increase of the group of anthocyanidins in comparative examples 1-4 causes the intelligent membrane to be rough in section, which is probably because the anthocyanidins are poor in compatibility with PVA and starch and are aggregated to form lumps; the film sections of the groups 1 to 4 and the control group of the invention are rough, because the anthocyanin and the LAE are gathered in the film to influence the interaction between PVA and starch, so that the compact film structure is damaged, and a small amount of holes are formed in the film.
2. Fourier transform infrared spectroscopy
Grinding the composite membrane into powder by a file, wherein the ratio of the sample powder to the potassium bromide is 1:200, and fully and uniformly mixing in a mortar. Dehydrating in drying oven, and tabletting. Scanning range of infrared spectrum 4000-500cm-1Resolution of 8cm-1The scan signal is accumulated 32 times. The infrared spectrogram results are shown in FIG. 2.
FIG. 2 is an infrared spectrum of each set of composite films. As can be seen in FIG. 2, the O-H stretching vibration peak is 3280-3384cm-1And the C-H stretching vibration peak is near 2938cm < -1 >. -CH2The bending vibration peak and the C-O specific angle deformation peak in the phenolic compound are between 1412-1424 cm-1. The peak appearing around 1641-1656cm-1 is related to the starch bound water molecules. The C ═ C stretching vibration peak in the aromatic ring skeleton of the anthocyanin flavonoid compound is also between 1641-The characteristic peak is that the O-C stretching vibration peak of the hydrogen-free glucose ring in the anthocyanin flavonoid compound is about 1086cm < -1 >. The C-C and C-OH stretching vibration peaks in the PVA structure are near 1156cm-1, which is the PVA infrared characteristic peak. The C-O stretching vibration peak in the C-O-C group in the glucose ring of the starch is near 1008cm < -1 >, which is the infrared characteristic peak of the starch. The spectral lines in the upper figure are very similar, and the characteristic peaks are obvious, which indicates that the components are physically blended and no new chemical bonds are generated.
X-ray diffraction analysis
And (3) shearing the composite membrane into samples with the length and the width of 20mm, and fixing the samples on a sample table. The X-ray radiation source is CuKa, the wavelength is 15.4nm, the voltage is 40kV, the current is 15mA, the step length is 0.035 degrees, the scanning angle is 3-60 degrees, and the continuous scanning is 15 s. The X-ray diffraction analysis diagram is shown in fig. 3. The crystallinity of the composite film is calculated by MDIJade software, recorded in Table 1, and calculated by a relative area method according to a formula:
degree of crystallinity (%) ═ Sc/(Sc + S) × 100% (1)
In the above formula (1), ScIs the area of the crystalline region, and S is the area of the amorphous region.
TABLE 1
Note: the different upper case letters in the same column of data represent significant differences between samples (p ≦ 0.05); if the upper lower case letters are not added, the data have no significant difference (p > 0.05).
FIG. 3 is an X-ray diffraction pattern of each set of composite films. It can be seen from table 1 and fig. 3 that no significant change occurred due to the addition of anthocyanin. The diffraction peak of the pure anthocyanin is 20.30 degrees, and the diffraction peak positions of all the films are near 19-20 degrees, because the crystal structure of the tapioca starch is destroyed after gelatinization, and the composite film mainly has a PVA crystal structure. As shown in Table 1, as the content is increased, the crystallinity is reduced, which is related to the influence of anthocyanin on the ordered arrangement of PVA and tapioca starch, and the anthocyanin forms aggregates with crystallization characteristics, which indicates that the crystallinity of the composite film can be related to the type of anthocyanin, the type of additive, the preparation process and the selected base material.
4. Thickness and mechanical properties
The thickness was measured at 6 positions (1 in the center and 5 at the edge) on the composite film and averaged.
The composite film is cut into rectangular test sample strips with the length and the width of 60mm and 20mm respectively, the length of a stretched area of each test sample strip is 30mm, and the stretching speed is 10 mm/min. The results are shown in Table 2.
TABLE 2
Note: the different upper case letters in the same column of data represent significant differences between samples (p ≦ 0.05); if the upper lower case letters are not added, the data have no significant difference (p > 0.05).
As can be seen from table 2, as the content of anthocyanin increases, the tensile strength and the elongation at break of the composite film both show a trend of increasing and then decreasing. The tensile strength of the composite film is slightly reduced by adding LAE, the tensile strength of the film without adding anthocyanin is 20.95MPa, the elongation at break is 384.43%, when the content of anthocyanin is 5%, the maximum tensile strength is 24.43MPa, the maximum elongation at break is 439.25%, and when the anthocyanin is continuously added to 50%, the tensile strength is reduced to 11.25MPa, and the elongation at break is reduced to 103.02%. When the content of the anthocyanin is lower than 20%, the tensile strength and the elongation at break are both reduced after being slightly increased, and the difference is not obvious. Therefore, the addition of a small amount of anthocyanin (less than or equal to 20%) can not generate obvious influence on the mechanical property of the composite film, because the small amount of anthocyanin can be uniformly dispersed in the film, so that the interaction between PVA and tapioca starch is maintained or slightly enhanced, and the mechanical property is kept unchanged or slightly improved. And is higher than the low-density polyethylene film commonly used in the market at present.
5. UV blocking, light transmittance and opacity
The composite film was cut into rectangular test strips with a length and width of 40mm and 10mm, and fixed in a sample cell, and the ultraviolet shielding performance was measured in the wavelength range of 200-plus-400 nm ultraviolet light, and the transmittance and opacity of the film were measured in the 400-plus-800 nm visible light region, and recorded in table 3. FIG. 4 is a composite film versus color disk shading. The opacity calculation formula is:
opacity (-logT)600)/H (2)
T in the above formula (2)600The light transmittance of the composite film at the wavelength of 600nm is shown, and H is the thickness of the composite film.
TABLE 3
Note: the different upper case letters in the same column of data indicate significant differences between samples (p ≦ 0.05).
From table 3, it can be found that the light transmittance is reduced with the increase of the content of anthocyanin, and the blank group is not added with LAE and anthocyanin, and the ultraviolet transmittance is higher because PVA and starch cannot block ultraviolet rays; the transmittance of the other components to ultraviolet rays is 0%, which shows that the composite film containing LAE or anthocyanin has better ultraviolet ray blocking effect, LAE is easy to gather in the film to block the passage of ultraviolet rays in the film, and anthocyanin can well absorb ultraviolet rays, and the transmittance of the ultraviolet rays with the wavelength of 400nm in the group of the embodiment 1 is only about 13%, because the anthocyanin can absorb ultraviolet rays, and meanwhile, the gathering of LAE can also block the light passage; in food packaging, the ultraviolet-resistant packaging film has strong ultraviolet-resistant performance, is beneficial to prolonging the shelf life of food, reducing oxidation and better preserving the nutrition, flavor and color of the food.
In the visible region (400-800nm), the transmittance of the composite film containing LAE is slightly lower than that of the film without LAE. At the wavelength of 800nm, the light transmittance of the film without LAE is 77.84%, and the light transmittance of the composite films with different LAE contents is 74.53%, 74.25%, 42.80% and 72.54%, respectively. In general, as the LAE content increases, the film transmittance decreases slightly, which may be related to the aggregation of LAE, more LAE tends to form larger aggregates, thereby obstructing the passage of light in the film. The barrier property to visible light also plays an important role in food preservation, and can prevent vitamins and pigments from degrading and organic matters from being oxidized.
FIG. 4 shows the shielding of the color disk by each set of composite films. As seen by naked eyes in FIG. 4, as the content of anthocyanin increases, the color difference becomes obvious and the transparency decreases. But the film with no added anthocyanin and 5% added anthocyanin has the opacity value less than 5, which indicates that the film is transparent.
6. Water absorption and water vapor transmission
Cutting the composite film into samples with the length and the width of 20mm, heating a constant-temperature electric heating drying box to 50 ℃, putting the samples into the constant-temperature electric heating drying box for 24 hours, drying the samples to constant weight, weighing and recording the weight as M1. The dried sample was stored in a closed desiccator (containing a saturated NaCl solution, 25 ℃) at a relative humidity of 75% for 24 hours, taken out and weighed as M2And calculating a formula:
water absorption (%) - (M)2-M1)/M1×100％(3)
In the above formula (3), M1As initial weight of sample, M2The weight of the sample after water absorption.
Using the method of ASTM E96-00, a beaker (30 mL of deionized water at 100% relative humidity) 50mm in diameter was covered with a film 60mm in diameter and completely sealed with petrolatum to prevent water evaporation from the joint gap. Then weighing the whole weight of the beaker, putting the beaker into a closed dryer filled with 1kg of silicon dioxide, storing the dryer in a constant-temperature electric heating drying oven at 25 ℃, and weighing the whole weight of the beaker once every 3 hours until the weight is stable. Recorded in table 4. The water vapor transmission rate is determined by the relation between the whole weight reduction of the beaker and the used time, and the calculation formula is as follows:
water vapor transmission rate (g.m)-1·s-1·Pa-1)＝(dW×H)/(dt×dP×S) (4)
In the above formula (4), dW is the total weight loss of the beaker (g), H is the average film thickness (m), dt is the time change (S) under the partial pressure gradient of water vapor (dp 2533Pa), and S is the water permeation area from the film (m)2)。
TABLE 4
Note: the different upper case letters in the same column of data indicate significant differences between samples (p ≦ 0.05).
As can be seen from Table 4, the intelligent film with more anthocyanin is higher in water vapor transmission rate, but the indexes of each group are almost not different significantly, and after 24 hours, the water vapor transmission rate of the blank group is 4.79 multiplied by 10-12g·m-1·s-1·Pa-1Comparative examples 1 to 4 all had water vapor transmission rates of 9.29X 10-12g·m-1·s-1·Pa-1Above, the maximum can reach 1.16 multiplied by 10-11g·m-1·s-1·Pa-1(ii) a The water vapor transmission rate of the control group was 1.03X 10-11g·m-1·s-1·Pa-1The water vapor transmission rates of examples 1 to 4 were all 1.62X 10-11g·m-1·s-1·Pa-1The above. This is because more anthocyanins are agglomerated, which destroys the structural integrity of the film and promotes the transmission of water molecules, thereby slightly increasing the water vapor transmission rate. The water absorption of the intelligent film added with more anthocyanin is higher, but the indexes of each group almost have no significant difference, the water absorption of the blank group is 16.00 percent, and the water absorption of the comparative example 4 is 20.51 percent; the water absorption of the non-control group was 14.81%, and that of example 4 was 17.65%. This phenomenon occurs because anthocyanins contain more hydrophilic groups, resulting in a slight increase in water absorption.
7. In vitro bacteriostatic performance test
The composite membrane was cut into a sample having a diameter of 8mm with a puncher while preparing a TSA plate medium using a 90 mm-diameter petri dish, and the sample and the TSA plate were sterilized by ultraviolet irradiation for 2 hours in a sterile operating table. Then respectively take 108CFU/mL E.coli and S.aureus TSB ligationSeed 0.1mL, evenly spread on TSA plate. And finally, placing the sample on the surface of a TSA flat plate, placing the TSA flat plate in a constant-temperature incubator at 37 ℃ for 24 hours, and measuring the diameter (mm) of a bacteriostatic circle around the sample to evaluate the antibacterial activity of the composite membrane. Recorded in figure 5 and table 5.
TABLE 5
Note: different upper case letters in the same column of data indicate significant differences between samples (p ≦ 0.05).
FIG. 5 shows the inhibition zone of each composite membrane on Escherichia coli. FIG. 6 shows the inhibition zone of each composite membrane against Staphylococcus aureus. As can be seen from FIGS. 5 and 6 and Table 5, the blank group and comparative examples 1 to 4 have no inhibitory effect on bacteria, the agar plates are full of Escherichia coli and Staphylococcus aureus, no zone of inhibition occurs, and the anthocyanins used in the present invention may not have an inhibitory effect. The composite membranes of the embodiments 1 to 4 of the invention have obvious bacteriostatic zones and all have antibacterial effects.
8. Analysis of anthocyanin solution color with pH change
The anthocyanin and anthocyanin/LAE mixed solutions were tested for color change at different pH values (2-11) and recorded in FIGS. 7 and 8.
FIG. 7 is a graph of the color change of an anthocyanin solution at various pH values. FIG. 8 anthocyanin/LAE solutions change color at different pH values. As shown in fig. 7 and 8, in the anthocyanin solution, when the pH is 2 under acidic conditions, the solution is peach-red; when the pH was 7 under neutral conditions, the solution was grey; when the pH was 11 under alkaline conditions, the solution was light yellow-brown. In the anthocyanin/LAE solution, when the pH is 2 under acidic conditions, the solution is peach red, slightly deeper than the pure anthocyanin solution; when the pH was 7 under neutral conditions, the solution was grey; when the pH was 11 under alkaline conditions, the solution was dark gray. Under acidic conditions (pH 2-6), the two solutions were relatively close in color, and under alkaline conditions (pH 8-11), the solutions were slightly different in color due to the interaction of anthocyanins and LAE. The solution was peach-red when in acidic conditions, because there were only basic salt ions in the solution; when the solution gradually becomes neutral, the color gradually changes from pink to light pink until becoming light gray, because the basic salt ions lose protons, and quinone cations with blue color are formed; when the solution becomes basic, the pseudo-basic methanol structure is gradually replaced, forming a chalcone structure with a yellowish-brown color.
9. Color change of composite membrane under different pH values and application of composite membrane in delaying milk decay
Cutting the film into rectangular samples with the length and the width of 20mm, putting the samples into a culture dish with the diameter of 90mm and containing 30mL of fresh milk, placing the samples in a room temperature environment for 7 days, and observing the milk spoilage and the color change rule of the film.
FIG. 9 is a graph of the color change of the composite membrane of comparative example 1 at different pH values. FIG. 10 the color of the composite membrane of example 1 of the present invention changed at different pH values. As is apparent from fig. 9 and 10, the color of the composite membrane of comparative example 1 hardly changes at different pH, while the color of the composite membrane of example 1 changes more obviously.
Figure 11 initial colour of milk before soaking experiment. Figure 12 color profiles of each set of membranes were taken after the soaking experiment. FIG. 13 color change of milk after soaking experiment. As can be seen from FIGS. 11 to 13, the composite films of the blank group and the comparative examples 1 to 4 before and after soaking had almost no change in color, and the composite film of example 1 had a more marked change in color. FIG. 13 the white blank and comparative examples 1-4 groups changed color, caked, and developed a large number of microorganisms after 7 days, with significant mildew, and measured pH of 3.3; examples 1-4 milk changed color and caked after 7 days, but did not show too many microorganisms, did not mildew significantly, and measured pH was also 3.3, which indicates that the composite membrane obtained by the method of the present invention has an inhibitory effect on microorganisms, and can retard or prevent the growth of microorganisms.
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (9)
1. A preparation method of a PVA/cassava starch/LAE/anthocyanin intelligent color-developing active composite membrane is characterized by comprising the steps of gelatinizing cassava starch, mixing the gelatinized cassava starch with a PVA solution and glycerol, adding LAE accounting for 1-5 wt% of the total mass and anthocyanin accounting for 5-50 wt% of the total mass, stirring and mixing uniformly under the heating condition of a constant-temperature water bath to obtain a membrane casting solution, and finally carrying out a tape casting method on the membrane casting solution to obtain a finished product composite membrane.
2. The preparation method of the PVA/tapioca starch/LAE/anthocyanin intelligent color-developing active composite membrane according to claim 1, which is characterized by comprising the following steps:
(1) gelatinized tapioca starch
Adding cassava starch into deionized water to prepare a starch suspension with the mass concentration of 10-11%; putting the starch suspension into a constant-temperature water bath environment, heating to 81-84 ℃, and stirring for 30-35 min until the starch suspension is completely gelatinized to obtain gelatinized starch for later use;
(2) preparation of PVA solution
Putting PVA into deionized water according to a certain solid-liquid ratio, placing the PVA into a constant-temperature water bath environment, heating to 98-100 ℃, and stirring for 54-58 min until the PVA is completely dissolved to obtain a PVA solution with the concentration of 10-11%;
(3) preparing casting solution
Mixing gelatinized starch and a PVA solution according to a volume ratio of 70: 30-32 to obtain a mixture 1, adding glycerol into the mixture 1 to obtain a mixture 2, placing the mixture 2 in a constant-temperature water bath environment, heating to 81-84 ℃, and stirring for 30-35 min to uniformly mix the solutions to obtain a mixed solution for later use;
adding LAE accounting for 1-5 wt% of the total mass of the mixed solution and anthocyanin accounting for 5-50 wt% of the total mass of the mixed solution, continuing stirring in a constant-temperature water bath environment at 23-25 ℃ for 30-33 min until all components are uniformly mixed, taking out, and placing in an ultrasonic environment to vibrate at normal temperature for 4-5 min to obtain the membrane casting solution;
(4) casting film by tape casting method
Pouring the casting solution into a mould by adopting a tape casting method for casting, then placing the mould in a constant temperature environment for drying and demoulding to obtain a composite membrane, and sealing and storing the composite membrane.
3. The preparation method of the PVA/tapioca starch/LAE/anthocyanin intelligent color-developing active composite film according to claim 2, wherein the composite film has a thickness of 0.11-0.18 mm, a tensile strength of 11.25-24.43 MPa, an elongation at break of 103-439%, a light transmittance of 0 at 200nm, an opacity of 4.11-11.01, a water absorption of 15.79-17.65%, and a water vapor transmittance of 1.00 x 10-11～1.62×10-11g·m-1·s-1·Pa-1。
4. The preparation method of the PVA/tapioca starch/LAE/anthocyanin intelligent color-developing active composite membrane as claimed in claim 2, wherein the stirring is carried out at a speed of 425-430 r/min.
5. The preparation method of the PVA/tapioca starch/LAE/anthocyanin intelligent color-developing active composite membrane as claimed in claim 2, wherein the addition amount of the glycerol is 18-20% of the total dry weight of the mixture 1.
6. The preparation method of the PVA/cassava starch/LAE/anthocyanin intelligent chromogenic active composite membrane according to claim 2, wherein the anthocyanin is mulberry anthocyanin; and (3) adding anthocyanin in an amount which is 5 percent of the total mass of the mixed solution.
7. The preparation method of the PVA/tapioca starch/LAE/anthocyanin intelligent color-developing active composite membrane according to claim 2, wherein the drying temperature in the step (4) is 25-28 ℃, and the drying time is 24 hours.
8. A PVA/cassava starch/LAE/anthocyanin intelligent color development active composite membrane obtained by the preparation method of any one of claims 1 to 7.
9. The application of the PVA/tapioca starch/LAE/anthocyanin intelligent chromogenic active composite membrane in packaging bacteriostasis according to claims 1-7, wherein the composite membrane has bacteriostasis to escherichia coli and staphylococcus aureus and can be used as a packaging material in food and pharmaceutical products.
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